Eduaed ulleich



UNITED STATES PATENT OFFICE.

EDUARD ULLRIOH, OF HQOHST-ON-THE-MAIN, ASSIGNOR TO CARL ROTH, OF BERLIN,AND THE FARBWERKE, VORMALS MEISTER, LUCIUS & BRUNING, OFHCOHST-ON-THE-MAIN, GERMANY.

PRODUCTION OF DIETHYLMETHYLTHlONlN-BLUE.

SPECIFICATION forming part of Letters Patent No. 366,640, dated July 12,18L'7.

Application filed January 13, 1887. Serial No. 124,2?3.

(No specimens.) Patented in France December 24, 1885, No. 173,137;

in Germany December 25, 1885, No. 38,573, and in England January 1,1886, No. 43.

.To all whom, it 7720.1 concern.-

Be it known that I, EDUARD ULLRIoH, doctor of philosophy, a citizen ofthe Empire of Germany, residing at I'Iochst-on-the-Main, in the Empireof Germany, have invented certain new and useful Improvements inDiethylmet-hylthioniirBlue; and I do hereby declare the following to bea full, clear, and exact description of the invention, such as willonable others skilled in the art to which it appertains to make and usethe same.

This invention relates to a blue coloringmatter or dyestuff, which Iterm diethylmethylthionin -blue, the hydrochlorate of O H,N(O,H,)diethylmcthylt-liionin N S 0,11 4 NH(GH,) Ge being an essentialconstituent of the same. This blue coloring-matter I produce by jointoxidation of paramido-diethylaniline (1)N(O.,H,l, l andmonomethyl-aniline in presence ofa hyposulphite, and precipitating thecoloring-matter from its solution by means of chloride of zinc andcommon salt.

According to the said inventiou,ilfteen parts of diethylaniline aredissolved in diluted hydrochloric acid (forty parts of water andsixty-five parts of concentrated hydrochloric acid) and then by sevenand one'tenths parts of nitrite of sodium, and subsequent addition ofzinc converted into amido-diethylaniline. Zinc is added in the quantitynecessary to use up all the free hydrochloric acid. The solution thusobtained is diluted with water to about five hundred parts, and then areadded fourteen parts of hydrochlorate of monomethylaniline andtwenty-five parts of hyposulphite of sodium. Now I oxidize by ad- 0 dinga solution of twenty-five parts of potassium dichron'late, boil forabout two hours, add the quantity of sulphuric acid necessary to bindthe ehromoxide and the alkalies, and expel the sulphnrons acid byfurther boiling. 4.5 Then the dissolved leuco compound is converted intothe coloring'matter by the addition of an oxidizing agent, and finallyit is precipitated by means of common salt.

The coloring-matter is a brown powder of 50 bronze-like appearance. Theblue solution of the same is easily reduced to a colorless liquid, theoriginal shade of which is restored by oxidizing agents. By means oftannin and emetic tartar the coloringmatter is fixed on 5 the fiber sothatit will resist washing. Quicksilver chloride and potassiumdichromate precipitate the solution. The precipitate is of a dark-blueshade. L

Vhat I claim as new, and desire to secure by 60 Letters Patent, is'

As a new product, diethylmethylthioninblue produced by joint oxidationof paramidodiethylanilincand 1nononicthyl-aniline in presence of ahyposulphitc, and having the char- 65 acteristics above set forth.

In testimony whereof I affix my signature in presence of two witnesses.

EDUARD U LLRIOH.

\Vitnesses:

JEAN GRUND, JACOB M UELLER.

